Calorimeter.



S. W. PARE.

CALORIMETER.

APPLICATION FILED MAY 6. 1914.

2 SHEETS-SHEET 1.

j? as l u?" Ri gf Samuel W. 'Daur 3513 futon/leg w m w m Patented Apr. 20, 1915.

s. w. PAAR.

2 SHEETS-SHEET 2.

I i 4f ZJ 4l f l v I f f s y e\\/I 24 I /6 4I/11111111111111101111!) L 78 .50 Y' v77 g1/wauw@ Samuel W. Parr w13 @Hom/lud Patented A101220, 1915,

lili

hpecieation of Letters lPatent.

rarement am. eo, mit.;

dimplication led May 6, wie. Serial No. 336,625.

To all whom t may concern Be it known that-l, SAMUEL W. Penn, a citizen of the United States, residing at Urbana, county of Champaign, State of illinois, have invented certain new and useful improvements inpCalorimetex-s; and l' do hereby declare the following to be a full, clear, and exact description or' the invention, such as will 'enable others skilled in the art to which it appertains to make and use the same. Y

rllhe present invention relates to calorimeters and more particularly to apparatus for use in determining the caloriiic value of coal and similar combustibles.

llt is the object of the present invention to provide an apparatus in which the combustible charge is permitted to attain a high temperature throughout until the combustion is substantially complete, but with means for quickly absorbing the heat thus developed. l

More particularly, it is the object of the presen-t invention to protect the combustion chamber from vcontact with the water or other cooling liquid in which it is immersed until after the'combustion is well under way or even is complete, and thereafter to bring the combustion chamber directly in contact with the cooling liquid to edect quick transference of its heat and that of the combustion products which it holds.

rlhe apparatus of my invention possesses various structural features of importance, the objects and advantages of which will be made clear by the following detailed description, which is to be takenl in conjunction with the accompanying drawings, wherein- Figure 1 is a sectional elevation through the containers showing the calorimeter in side elevation; Fig. 2 is a partial side elevation of the container illustrating the spring contact member at its top; Fig. 3 is a section through the calorimeter portions of the driving pulley being broken away; Fig. 4 is a sectional plan on -the line 4 4 of Fig. 3; Fig. 5 is a section on the line 5-5 of Fig. 3; and Fig. 6 is an enlarged detail of the electrical contact at the base of the fluid holding vessel. l

lin the embodiment illustrated, the apparatus comprises an outer container land an inner container 2 spaced apart Yto forma deadeair'space 3 and'se'cured together asoby means of a screw 4; with cork-'spacing washers 5. These containers may be of in. durated fiber, or other material of low heat conducting capacity, and are provided with a double air insulated cover comprising disks 6 and 7 held together by screws 8 and spacedapart by washers of cork, felt or the like. Witlnn the innercontainer and spaced therel fromby supporting blocks 9 is a vessel l0 containing water, or other suitable cooling liquid, wherein the calorimeter may be imniersed when`combustion of its charge is to be eected. rllhis vessel 10 is preferably of metal and is tted with atubular deflector 11 cut away at its bottom to form fluid passages 12 through which circulation of the water may be eected. Supported in this deiectoris a cross-bar 13 having arms 14 contactin with the walls of the vessel 10 and serving to center the deflector in the vessel. At the center of bar 13 is a pivot whereon the calorimeter may rest and may be rotated.

At the side of the louter container l is a pair of electrical terminals 15, one of which is connected througha copper strip 16 with the contact device shown in detail in Fi 6 as comprising a tubular socket 17 threa ed to receive a nut 18 whereby the copper strip 16 may be held in place, and containing a spring pressed plunger 19 adapted to bear yieldingly against the bottom of, the metal vessel 10 to establish electrical connection therewith. The other terminal is connected with a' plate 20 secured to container 1 and pivotally supporting a spring-arm 21 bear-ing'a thumb-piece 22, and shaped so that it can be pushed down into contact with the top of the rotating element of the calorimeter to establish the flow of current therethrough for purposes hereinafter set forth. A thermometer 23 passes through the covers and has its bulb positioned in the annular space between vessel 10 and deflector 1l at about the level ofthe calorimeter.

The calorimeter itself comprises a seamless metal cup 2li, preferably of nickel-'iron alloy 'of about the composition 70 per cent. iron and per cent. nickel. ln operating the calorimeter by the peroxid method, hereinafter disclosed, a hlghly corrosive alkalinefusion is formed in the cup, and any corrosive action which it may vhave on'the cup not 'only shortens the life of the latter, but also introduces an element of error in the heat readings. ll have found that a nickel-iron alloy fof 'the composition above tot l stated is much more resistant`than pure nickel or 'most of the metallic elements, and is well suited for use in the construction of this part of the calorimeter. The chamberrwalls are of uniform thickness throughout, except at the upper edge, where they are shaped to form a shoulder 25 and an outwardly extending flange 26, the upper face of which is smooth and level to receive a gasket 27. Inclosing the` combustion chamber is a cylindrical metal casing, the upper edge ofi which has an annular recess 28 to receive flange 26, and the extreme upper edge of which is in the form of an annular tongue overlapping the edge of flange 26 and lying flush with the top face thereof and in intimate contact with gasket 27, which serves, therefore, not only to seal the combusion chamber,l but also to seal the joint between the combustion chamber and itsy inclosing casing.

The combustion chamber is provided with a cover 29, preferably of the same` nickeliron alloy, this cover having its central portion shaped to enter the combustion chamber with a snug 't and for a distance far enough to protect gasket 27 from the- Vapors and products of combustion developed .in the chamber. `With this arrangement, gasket 27 may be of rubber, `and this I have found to be a great con.- venience. The gasket lies in an annular recess in cover 29 andthe eXtreme outer edge of the latter'is in theform of an annular lip 30 which overlaps the upwardly ex! tending tongue of the casing, thereby protccting the rubber gasket from squeezing out laterally, and in other ways contributing to the security of the joints.

Cover 29 carries an integral, tubular stem y31, the lower portion of which is provided with a tapered hole to receive an insulating gasket 32 of rubber, or the like, wherein is fitted a tapered socket 33 threaded to a conducting rod 34, which passes upward through stem 31 and is attached by means of a nut 35 to afhub 36 whereon a driving pulley 37 may be mounted for rotating they calorimeter in its bath when desired. The nut 35 is of. conical outline and coperates with the spring contact arm 21, as shown in Fig.\2. An insulating bushing 38A of -rubber, or the like, isV interposed between the pulley and the main portion of the stem, not onlv to electrically insulate the two parte, but also to prevent the escape of heat upward through the stem to the pulley.

useof a fuse-wire39, one end of which is 65- connected to a terminal v40 screwed directly Whengthe apparatus is in use,vbushing 38 lies atv about the level of the container tops and keeps substantially all of the heat withp in the containers, .where it can be measured.

As a means forigniting the combustible charge 1n the' combustion chamber, I make into cover 29, and the other end of which is connected through a similar terminal 41, the shank of which lis screwed into sleeve 33, and holds an insulating disk 42 over the conical opening in cover 29.

Each of the terminals has a hole and an inclined slot opened at its upper or outer end to form a notch, and in mounting the fuse-wire on the terminals, its end is pushed through the holeA for about 1/4 of an inch and then bentsharply down against the face of the terminal. The remainder of the wire is then Wound two or three times around the terminal at the` narrow part formed by the slot binding in the short end passed throughthe eyelet, and finally the wire is bent downward in line with the terminal to form a loop from the other terminal similarly strungup. With this arrangement there is certainty of electrical contact between the use-wire and the terminals, and the construction is rugged and well adapted to withstand the high temperatures and corrosive conditions present in this type of apparatus. Preferably, the terminal blocks are made of the above mentioned nickeliron alloy.

The upper portion of the casing is screwthreaded to receive a cap 43, which overlaps the top of cover 29 and serves to hold it tightly in position with its gasket 27 under compression. The outer face of this screw cap may be of octagonal outline, as shown in Fig. 5, to serve as a wrench seat, whereby the cap may be screwed into place. The central portion 44 of the casing is similarly provided with an octagonal wrench seat, whereby'it may be held while the cap is being screwed into position. Mounted on the lower portion of the casing is a spring-band 45 carrying paddles 46, so that when the apparatus is rotated, a circulation of the cooling water will be effected.

The casing which incloses combustion chamber 24 is spaced therefrom tc form an annular air chamber about 1/64 of an inch across and extending-` throughout substantially the entire length of the combustion chamber. The bottom of the casing is pro vided witha flange 47 above which is a metal bottom 48 which may be called a floatingV bottom, in the sense that it may move upwarduntil 'its 'central pedestal 49 contacts with the bottom of the combustion chamber. Pedestal' 49 has a height of from 1/32 to 3/32 of an inch, so that when thus in contact it leaves an additional air space combustion-cup when the apparatus is subatinente i ground to 60 or 100 mesh,` 1 grm., of potassium clilorate, KClUB, and, approximately, 10 grms. of sodium peroxid of standard strength. The coal and potassium chlorate are weighed carefully and the sodium peroXid is measured. When the mixture -is in the combustion chamber, and tightly sealed up with the fuse-wire in place, the apparatus may be shaken to e'ect thorough mixture of the charge, and the calorimeter may then be lowered into the water until the floating bottom strikes the pivot and is forced up intoy contact with the bottom ofv the calorimeter. At this stage of the operation, the co1nbustion chamber is enveloped substantially throughout in aprotective layer of air lying inthe narrow space between the casing and the combustion chamber. v 4

After rotating the apparatus until the temperature conditions have become constant, a suitable voltage may be applied to terminals 15 and the spring contact arm 21 may beforced down into contactwith terminal 35, thereby passing current through the fuse-wire and through the calorimeter to the pivot-bar 13, from which it passesl down by way ofthe spring-pressed contact 19 and finally tothe other terminal 15. vThe momentary flow of current will burn the fuse and-ignite ythe charge, and the reaction Will go on in accordance with the principles and method set forth at length in my Patent No. (373,325, issued April 30, 1901. During the initial stages of the reaction and while the temperature of the combustion chamber is going up, the 'air immediately surrounding the combustionchamber will be expanded and forced out through the small holes 50,

and under these conditions there is no chilling of the charge through eontact with the walls of the container, and substantiahy` complete ignition and-combustion results; but as soon as the charge begins to cool, the contraction o f the airpermits the entry of water, and this is drawn into cont-act' with the combustion chamber and finally rises almost to the top of the annular lair space between the, casing and the combustion chamber. By thus bringing the water into intimate contact with the combustion chamber, 'as soon as the combustion is. substantially complete,` a quick transference of the heat is effected, and there is no need to wait for its slow transference through a dead air space or upward to the top of the combustion chambenivvhere it is in contact with the other metal parts. The heat transference is substantially complete yat the end of :fourA or tive minutes, whereas if the heat wei'efcompelled to pass across the air space, or',by conf duction, up through the points of contact at the upper edge `of the cup, ythe timerequired would amount to. from ten to twentyyinin- Intes, and this would ,permitl errors inadmissible in practice. y e

` rWliilethe combustion is going on, theapf, parats is steadily rotated by means of its" pulley iland circulates ,the water, or other cooling liquid', through the openings 12 in shield 1l -and upward around the calorime ter, so that it may pass down again between the deflector and the vessel 'to complete theA circulation. After the thermal determinations are complete, and the calorimeter has been removed from the water, its screw-cap isturned off with' a wrench and the cover liftedout, after which the floating bottom 48 can be forced'up to'lift the calorimeter out of its casing for further treatment of the residue. rfhis enables the operator to take hold of the outside of the cup and not ycontaminate the residue of the charge by putting his fingerson the inside of the vcup where theywould'be brought 'in contact with the condensed alkali'vapors produced incidental to the foregoing process. After removal of the combustion chamber, the bottom 48 may be taken out entirely and the entire apparatus may be thoroughly wiped out and dried,and made ready for furtheruse.

Iclaim: W

1. ln a calorimeter, the combination of a combustion chamber, means for igniting a charge therein, a perforate envelop shielding said 'combustion chamber from the cooling @fluid until. combustion is well under way and thereafter permitting direct contact of the cooling fluid with the combustion chamber to-eifect rapid transference of theheat;

substantially as described.

l 2. lin a calorimeter adapted for immersion in a cooling liquid, the combination of a closed combustion chamber wherein. a charge may be ignited, and an envelop with an vairchambe'r protecting said combustion chamber from direct contact with the liquid luntil after combustion is substantially comd. In a calorimeter adapted for immersion iu'al cooling liquid, the combination of a closed combustion chamber wherein a charge may be ignited, a casing enveloping said combustion chamber with an air space intervening, and said casing having holes through which the heated air may escape while the temperature vof the combustion chamber is increasing-and through which water maybe drawn uin when the temperature of the combustion chamber begins to decrease, thereby producing quick transference of the heat of the burning charge to the cooling liquidin ing air gap,

which the calorimeter is immersed.

5. In a calorimeter adapted for immersion in a cooling liquid, the combination of a closed combustion chamber wherein a charge may be ignited, a casing enveloping said combustion chamber with an' intervens aid casing having a fioating bottom limiting the air space below the combustion chamber when the apparatus is mounted in position for ignition of the charge. l

6. In a calorimeter adapted for immersion in a cooling liquid, the combination of .a combustion chamber wherein a charge may be ignited, and a casing enveloping said combustion chamber with an intervening air gap, said casing having a removable bottom and having holes through which heated air may escape while the combustion chamber is increasing in temperature, and through which water may enter into direct contact with the combustion chamber when the temperature thereof is decreasing.

7. In a calorimeter, the combination of a combustion chamber, a casing secured theretact with the heated to and spaced from the body of the combustion chamber by a narrow air gap, a cover fitting down into said combustion chamber and having a recess, a rubbergasket in said recess serving as a gas-,tight clo- Sure for said combustion chamber and for said air gap, and a collar overlapping said cover and threaded to said casing, whereby the gasket may be held tightly to its seats.

8. In a calorimeter, the combination of a combustion chamber, a cover fitting down within said combustion chamber and ,having an annular recess, a rubber gasket in said recess seated on the upper edge of said combustion chamber, and a casing enveloping said combustion chamber and spaced therefrom to form an air gap, the upper edge of said casing contacting with said rubber gasket and means for holding in place said cover and its gasket.

9. In a calorimeter, the combination of a combustion chamber, means for sealing said combustion chamber with a rubber gasket while protecting the rubber from direct conproducts of combustion, a casing inclosing ber and spaced therefrom to form an enveloping air chamber, said chamber being said combustion cham-l Sealedby said rubber gasket, and said casing having air openings through which hot air may escape while the combustion chamber is increasing in temperature, and through which water may-be admittedsubsequently to quickly cool said combustion chamber.

l0. In a calorimeter, the combination of a combustion chamber, lhaving at its top an outstanding flange, a4 easing spaced from ksaid combustion chamber' and having its upper edge flush with the upper edge of the combustion chamber, a gasket seated on said upper edges and a cover for said lcombustion chamber having a recess for said gasket, said cover extending into the -combustion chamber far enough to protect said gasket from the hot products of combustion.. 11. In a calorimeter, the combination of a combustion chamber, having at its top a shoulder and -an outstanding flange, a cylindrical casing fitting against said shoulder" and having a recess receiving said flange, a coverfitted to said combustion chamber and provided with a rubber gasket protected by a part of said cover from direct contact with the products of combustion within the chamber, and a cap overlapping said cover and threaded to said casing, said cap and casing having wrench seats and said casing having air openings; substantially as described.

12. In a calorimeter, the combination of a combustion chamber, a casing inclosing said vcombustion chamber but spaced therefrom to form anv air gap, a cover fitting down within said combustion chamber and having an annular recess, a rubber gasketin said recess ylying against the upper edge of said Combustion chamber and against the upper edge of said casing, and a cap overlapping the top oi" the cover and in threaded engagement with said casing to hold the cover in place.

13. In a calorimeter, the combination of a combustion chamber, a cover therefor, a gasket between said cover and said chamber, a casing inclosin said combustion chamber and spaced there rom to form an enveloping air chamber, sa-id casing having openings through which heated air may be expelled as said combustion chamber heats up, and through which a cooling fluid may be drawn when the combustion chamber begins to cool, and a cap threaded to said casing and holding the cover of said combustion chamber in place.

14. In a calorimeter for use in the combustion of coal in the presence of a pcroxid, a closed combustion chamber and means for igniting a charge therein, said combustion chamber consisting essentially of 7 O per cent. iron and 30 per cent. nickel; substantially as described. c l

15. In a calorimeter .for the oxidation of coal by sodium peroxid, a closed combustion chamber and means for igniting a charge Lianne@ therein, the exposed metal within said combustion chamber being an alloy of about 70 parts iron and 30 parts nickel.

16. ln a calorimeter adapted for immersion in a cooling fluid, the combination of a combustion chamber, a cover therefor, means for holding said cover in place, said Cover having a stem whereby the calorimeter may be rotated in a cooling liquid, a driving pulley supported by said stem and a heat insulating bushing in saidv stein below said driving pulley.

17. 1n a calorimeter adapted for immersion in a cooling liquid, the combination of a combustion chamber, a cover therefor having a hollow stem, an electrical conductor passing through said stem for ignition of the charge within the combustion chamber, a pulley mounted onsaid stem whereby said calorimeter may be rotated in a cooling liquid, and heat insulating means between said pulley and said combustion chamber to limit the conduction of heat through said stem to said pulley.

18. 1n a calorimeter adapted for rotation in a cooling fluid, and having an upright stem, the combination of a pulley mounted on said stem and whereby said calorimeter may be rotated, and a heat insulating bushing between said pulley and the main portion of said stem. y

19. 1n a calorimeter, the combination of a metal vessel for holding liquid, a tubular de- Hector therein having fluid openings near its base, a lsupporting pivot carried by said deflector, a calorimeter mounted to turn on said pivot and having paddles for establishing a circulation of cooling liquid throughout said deiector, there being an electrical connection to the body of said calorimeter through said deiector and vessel, and means for conveying current to the inside of said calorimeter for-ignition of a fuse-wire electrically connected with the body of said calorimeter.

20. lln a calorimetric apparatus, the combination of an insulating container, a Huid supported by said container and movable to establish an igniting circuit within said calorimeter while the latter is rotating.

21. ln a calorimetric apparatus, the combination of a calorimeter having an upright stem with a` conductor therein exposed at its top, a sealed insulating container enveloping said calorimeter and a yielding Contact arm supported by said container and movable into contact with said conductor to initiate a flow of current in said conductor; substantially as described.

Q2. ln a calorimeter, the combination of a closed combustion chamber wherein a charge may be ignited, a pair of terminals therein, one electrically connected with said combustion chamber and the other insulated therefrom, each of said terminals having an eye and having an inclined slot open at its upper end, and a fuse-wire wrapped entirely around said terminals at the slots and having its ends passed through the eyes and bound under said wrappings. y

23. 1n a calorimeter, the combination of a combustion chamber, a cover therefor, and a terminal threaded into said cover and having an eye throughwhich the end of a fusewire may be passed, said terminal also having an open notchv at which the fuse-wire may be wrapped entirely around the terminal to insure good electrical connection; substantially as described.

ln testimony whereof ll affix my signature, in presence of two witnesses.

SAMUEL W. PARR. lVitnesses:

JUSTA M. LINDGREN, FRED H. WHITTUM. 

